Hydrothermal synthesis and characterization of a new vanadyl sulfate compound: crystal structure of [V(IV)OSO4(H2O)4]·SO4·[H2N(C2H4)2NH2]
1999; Elsevier BV; Volume: 292; Issue: 1 Linguagem: Inglês
10.1016/s0020-1693(99)00153-x
ISSN1873-3255
AutoresM. Ishaque Khan, Sabri Çevik, Robert J. Doedens,
Tópico(s)Catalysis and Oxidation Reactions
ResumoThe hydrothermal reaction of a mixture of vanadylacetylacetonate-VO(acac)2, Na2SO4, piperazine, and diluted H2SO4 at 160°C gives a blue colored solution which yields rectangular blue crystals of [V(IV)OSO4(H2O)4]·SO4·[H2N(C2H4)2NH2] (1) in a 60% yield. Complex 1 is a new organic–inorganic compound: a vanadyl sulfate cocrystallized with organic species. The structure of 1 consists of layers of [V(IV)OSO4(H2O)4] separated by SO4 2− and doubly protonated piperazine cations [H2N(C2H4)2NH2]2+ which are hydrogen bonded with each other. Crystal data for 1: monoclinic, space group P21/c (no. 14), a=17.1502(10), b=7.2860(4), c=12.4448(7) Å, β=107.058(10)°, V=1486.7(2) Å3, Z=4. The structure was solved by direct methods and least-squares refinement converged at R=0.0305.
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